HRID2064157

反应详情

EQUATION

反应方程式

HRID 2064157 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A stirred solution of 2-bromo-4-fluorobenzotrifluoride (1.0 g, 4.1 mmole) in concentrated sulphuric acid (10 ml) at 0° C. was treated portionwise with KNO3 (0.46 g, 4.6 mmole) and maintained at 0° C. for 0.5 hr before warming to room temp. over 2 hr. The mixture was added to well stirred ice/water (100 ml) and then extracted with ethyl acetate. The extract was dried and concentrated under vacuum to afford the title compound as a yellow solid (1.2 g, 100%). 1H NMR (400 MHz, CDCl3) δ: 7.75 (1H, d), 8.45 (1H, d).

WORKUP

后处理

  1. temperaturebefore warming to room temp. over 2 hr
  2. extractionextracted with ethyl acetate
  3. customThe extract was dried
  4. concentrationconcentrated under vacuum